CN108048859A - A kind of electrolytic reduction for preparing graphene - Google Patents
A kind of electrolytic reduction for preparing graphene Download PDFInfo
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- CN108048859A CN108048859A CN201810153055.4A CN201810153055A CN108048859A CN 108048859 A CN108048859 A CN 108048859A CN 201810153055 A CN201810153055 A CN 201810153055A CN 108048859 A CN108048859 A CN 108048859A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
Abstract
The invention belongs to graphene preparation methods, and in particular to step 1 a kind of electrolytic reduction for preparing graphene, graphene oxide particle is put into distilled water, add in dispersant ultrasonic disperse, obtain graphene oxide dispersion；Step 2, graphene dispersing solution is added in into 3 5h of microwave compressive reaction into sealing reaction kettle, fine grained graphite alkene dispersion liquid is obtained after quick pressure releasing；Step 3, sodium chloride is added in fine grained graphite alkene dispersion liquid, adds in methanol and stir evenly rear 5 8h of cell reaction, obtain graphene dispersing solution；Step 4, by 1 3h of graphene dispersing solution ultrasonic disperse, then 1 3h of sealing pressing reaction, quick pressure releasing obtain graphene mixed precipitation；Step 5, graphene mixed precipitation is put into 1 3h of ultrasonic reaction in absolute ethyl alcohol, is dried after filtering and obtain grapheme material.The present invention solves the problems, such as that the method that existing electrolytic reduction prepares graphene has pollution with safe, and preparation method is simple and practicable, environment friendly and pollution-free.
Description
Technical field
The invention belongs to graphene preparation methods, and in particular to a kind of electrolytic reduction for preparing graphene.
Background technology
It is unique conductive possessed by graphene since acquisition high-quality graphene is removed using micromechanics stripping means
Heat conduction and mechanical performance attract scientific research circle and the great interest of industrial circle always.Due to excellent properties, the market of graphene
Demand is also increasing, this require grapheme material preparation constantly improve and can realize the technology of preparing of green non-pollution with
Obtain the graphene of high-volume high quality.However also there is very big challenge in current preparation in face of commercial application.First, may be used
Obtain high-quality graphene chemical vapour deposition technique and epitaxial growth method there are low yield, high energy consumption and transfer difficulties etc. to ask
Topic；In addition, although chemistry redox method can be realized prepares graphene on a large scale, there are a large amount of oxygen-containing groups to be connected to stone
On black alkene lamella, the electrical and thermal conductivity performance of graphene is caused to be greatly lowered.Moreover, ultrasonic stripping method and liquid phase shearing stripping method
The grapheme material of high quality can be obtained, also without using strong acid or strong oxidizer, and without metal ion, but obtained
Graphene lateral dimension is less than normal, it is most important that yield is very low, and often yield is less than 5%, and needs to be separated by filtration, economy
Difference, total cost performance be not still high.
For existing graphene preparation technology or the high cost of high quality or at low cost of poor quality, graphene industry
Develop there is an urgent need for it is a kind of can be mass-produced, the technology of preparing of high quality, low cost and green non-pollution, to break through grapheme material
Bottleneck.It is one of possible approach that electrochemistry, which prepares graphene,.Compared to oxidation-reduction method, Strong oxdiative is not required in electrochemical process
Agent instead electric field oxidation are removed；Compared to chemical vapour deposition technique, yield prepared by electrochemistry is far longer than gas
Phase deposition technique；The yield less than 5% compared to ultrasound or liquid phase shearing, electrochemical process can obtain the yield close to 100%.
However existing electrochemistry technology of preparing not enough or is not enough to the grapheme material for preparing high quality on a large scale.
In the electrochemistry having disclosed prepares the document and patent of graphene, used electrolyte can be divided into ion
Liquid, strong acid and some salting liquids.Wherein, the progress cathode using ionic liquid as electrolyte exists in the prior art to insert
Layer is removed, and can obtain the graphene that thickness is 2~3 layers, oxygen content is 2.5%, but when using ionic liquid as electrolyte,
The common problem encountered is that the expensive and complicated zwitterion impurity removal of ionic liquid is highly difficult etc., thus is difficult to industry
Change and use.In the prior art also there are a kind of technology of similar il electrolyte mechanism, particular by high-temperature heating chlorine
Change the salt such as potassium, sodium chloride, it is made to melt as electrolyte, the graphene defect of gained is few, low for equipment requirements, but high temperature item
Part energy consumption is higher, containing being difficult largely cleared ion such as chlorion, potassium ion and sodium ion etc. in obtained product, greatly
Ground influences the use of graphene.A large amount of sulfuric acid and glycine are used as electrolyte in addition, also existing in the prior art, although stripping
From speed quickly, can be completed in 5 minutes, and it is 2-5 layer of graphene that can obtain thickness, but equally exist be difficult to it is complete cleared
Sulfate radical and glycine ion.In addition, relatively environment-friendly and easy method is as electrolyte, example using some salting liquids
Such as, the electrolyte that solvation is made of lithium salts and propene carbonate exists in the prior art, makes lithium ion in electrolytic process
It is inserted into graphite layers to carry out removing acquisition graphene, but there are complicated for operation, electrolyte and foreign ion after stripping removals
The problem of very bothering and add the cost of industrialization.Similar electrolysis is also used in addition, also existing in the prior art
Liquid K2SO4Salting liquid is removed, and the voltage needed for this technology is relatively low, and required time is also shorter, but the product reacted can draw
Enter and be difficult to completely cleared metal ion, and sulfate ion equally understands partial oxidation of graphite alkene lamella, remaining sulfate radical
Compare and be difficult to remove.Moreover, also existing using ammonium sulfate as electrolyte in the prior art, the yield that this method obtains is up to
85%, the reaction time is short, but this method similarly faces the problem of sulfate ion can not be cleared, while sulfate ion
SO is also had in electrolytic process2Toxic gas generates, not enough environmental protection and safety.
The content of the invention
For the problems of the prior art, the present invention provides a kind of electrolytic reduction for preparing graphene, solves existing
There is the problem of polluting and is safe in the method that electrolytic reduction prepares graphene, preparation method is simple and practicable, can not only ensure
The high quality of graphene, and preparation method is environment friendly and pollution-free.
For realization more than technical purpose, the technical scheme is that：
A kind of electrolytic reduction for preparing graphene, the electrolytic reduction is in accordance with the following steps：
Step 1, graphene oxide particle is put into distilled water, adds in dispersant ultrasonic disperse, obtain graphene oxide
Dispersion liquid；
Step 2, graphene dispersing solution is added in into the microwave compressive reaction 3-5h into sealing reaction kettle, is obtained after quick pressure releasing
Fine grained graphite alkene dispersion liquid；
Step 3, sodium chloride is added in fine grained graphite alkene dispersion liquid, adds in methanol and stir evenly rear cell reaction 5-
8h obtains graphene dispersing solution；
Step 4, by graphene dispersing solution ultrasonic disperse 1-3h, then sealing pressing reaction 1-3h, quick pressure releasing obtain stone
Black alkene mixed precipitation；
Step 5, graphene mixed precipitation is put into ultrasonic reaction 1-3h in absolute ethyl alcohol, is dried after filtering and obtain graphene
Material.
Concentration of the graphene oxide in distilled water in the step 1 is 20-30g/L, the addition of the dispersant
It is the 10-15% of graphene oxide quality, the dispersant uses polyvinylpyrrolidone.
The dispersion frequency of ultrasonic disperse in the step 1 is 5-8kHz, and temperature is 40-60 DEG C.
The microwave power of microwave pressurization in the step 2 is 400-700W, and temperature is 120-150 DEG C, pressure 2-
5MPa, the speed of the quick pressure releasing is 0.5-0.7MPa/min.
Sodium chloride addition in the step 3 is the 30-50% of graphene oxide quality, and the methanol addition is to steam
The 50-60% of distilled water volume.
The voltage of cell reaction in the step 3 be 30-60V, electric current 30-90mA, 50-60 DEG C of temperature.
The supersonic frequency of ultrasonic disperse in the step 4 is 10-15kHz, and temperature is 80-90 DEG C.
The pressure of sealing pressing reaction in the step 4 is 20-30MPa, and temperature is 100-110 DEG C, described quickly to let out
The pressure release temperature of pressure is 90-100 DEG C, and pressure release speed is 1-2MPa/min.
Ultrasonic reaction in the step 5 is reacted using water bath sonicator, supersonic frequency 2-8kHz, and temperature is 60-70 DEG C,
Drying temperature in the step 5 is 80-90 DEG C.
Step 1 is added graphene oxide into distilled water, and it is suspended to be formed to the graphene oxide that distilled water is solvent
Liquid can be formed in surface of graphene oxide by the addition of dispersant and be adsorbed, play scattered effect, while be aided with super refreshing anti-
Should, it can disperse graphene oxide through a step using high-frequency vibration and clutch, and distilled water is acted on to graphene oxide
In gap, more careful suspended dispersion is formed.
Distilled water will be converted into water by way of microwave pressurization in graphene dispersing solution addition reaction kettle and steamed by step 2
Gas, and expansionization fragmentation is formed during quick pressure releasing, reach more careful graphene oxide refinement, while dispersant
Quick attachment can prevent graphene oxide from agglomerating again.
Step 3 adds in sodium chloride into solution for electrolyte, and adds in methanol as weak electrolyte, anti-by being electrolysed
Should, graphene oxide can be reduced in graphene, while the combination of weak electrolyte and strong electrolyte can not only ensure to be electrolysed
Effect ensures the progress of its reduction reaction, obtains stable graphene, while prevents the excessive decomposition for causing dispersant of electrolysis,
So as to pollute；The graphene of production can be kept scattered by dispersant.
Graphene dispersing solution is carried out ultrasonic disperse processing by step 4, can be by graphene dispersion；In sealing pressing process
In, methanol and distilled water are converted into gaseous state, good dispersiveness can be played and effect is filled up in gap, in quick pressure releasing process
In, using high temperature pressure release, gaseous solvent is quickly discharged, obtains the precipitation mixture with temperature.
Precipitation is put into ultrasonic reaction in absolute ethyl alcohol by step 5, can not only be disperseed precipitation mixture, be contributed to impurity
Dissolving, and ultrasound can promote absolute ethyl alcohol temperature, can increase solution rate and concentration of ordinary dissolution, ensure graphite olefinic impurity
Removal.
From the above, it can be seen that the present invention possesses advantages below：
1. the present invention solves the problems, such as that the method that existing electrolytic reduction prepares graphene has pollution with safe, preparation
Method is simple and practicable, can not only ensure the high quality of graphene, and preparation method is environment friendly and pollution-free.
2. the present invention as dispersant, can not only play dispersion effect using polyvinylpyrrolidone, at the same right and wrong from
Subtype high-molecular compound, it is with good stability, it can ensure its stability in electrolytic process.
3. the present invention ensures electrolysis effectiveness in a manner that strong electrolyte is mixed with weak electrolyte, while prevents electrolyte
Energy process causes electrolyte to aoxidize, and pollutes.
4. the present invention can all be dissolved the impurity in graphene as lytic agent using absolute ethyl alcohol, while graphene
It is insoluble, so as to promote the purity of graphene.
Specific embodiment
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to the claim of the present invention.
Embodiment 1
A kind of electrolytic reduction for preparing graphene, the electrolytic reduction is in accordance with the following steps：
Step 1, graphene oxide particle is put into distilled water, adds in dispersant ultrasonic disperse, obtain graphene oxide
Dispersion liquid；
Step 2, graphene dispersing solution is added in into the microwave compressive reaction 3h into sealing reaction kettle, is obtained after quick pressure releasing thin
Granular graphite alkene dispersion liquid；
Step 3, sodium chloride is added in fine grained graphite alkene dispersion liquid, adds in methanol and stir evenly rear cell reaction 5h,
Obtain graphene dispersing solution；
Step 4, by graphene dispersing solution ultrasonic disperse 1h, then sealing pressing reaction 1h, quick pressure releasing obtain graphene
Mixed precipitation；
Step 5, graphene mixed precipitation is put into ultrasonic reaction 1h in absolute ethyl alcohol, is dried after filtering and obtain graphene material
Material.
Concentration of the graphene oxide in distilled water in the step 1 is 20g/L, and the addition of the dispersant is oxygen
The 10% of graphite alkene quality, the dispersant use polyvinylpyrrolidone.
The dispersion frequency of ultrasonic disperse in the step 1 is 5kHz, and temperature is 40 DEG C.
For the microwave power of microwave pressurization in the step 2 for 400W, temperature is 120 DEG C, pressure 2MPa, described quick
The speed of pressure release is 0.5MPa/min.
Sodium chloride addition in the step 3 is the 30% of graphene oxide quality, and the methanol addition is distillation
The 50% of water volume.
The voltage of cell reaction in the step 3 be 30V, electric current 30mA, temperature 50 C.
The supersonic frequency of ultrasonic disperse in the step 4 is 10kHz, and temperature is 80 DEG C.
The pressure of sealing pressing reaction in the step 4 is 20MPa, and temperature is 100 DEG C, the pressure release of the quick pressure releasing
Temperature is 90 DEG C, and pressure release speed is 1MPa/min.
Ultrasonic reaction in the step 5 is reacted using water bath sonicator, supersonic frequency 2kHz, and temperature is 60 DEG C,
Drying temperature in the step 5 is 80 DEG C.
Embodiment 2
A kind of electrolytic reduction for preparing graphene, the electrolytic reduction is in accordance with the following steps：
Step 1, graphene oxide particle is put into distilled water, adds in dispersant ultrasonic disperse, obtain graphene oxide
Dispersion liquid；
Step 2, graphene dispersing solution is added in into the microwave compressive reaction 5h into sealing reaction kettle, is obtained after quick pressure releasing thin
Granular graphite alkene dispersion liquid；
Step 3, sodium chloride is added in fine grained graphite alkene dispersion liquid, adds in methanol and stir evenly rear cell reaction 8h,
Obtain graphene dispersing solution；
Step 4, by graphene dispersing solution ultrasonic disperse 3h, then sealing pressing reaction 3h, quick pressure releasing obtain graphene
Mixed precipitation；
Step 5, graphene mixed precipitation is put into ultrasonic reaction 3h in absolute ethyl alcohol, is dried after filtering and obtain graphene material
Material.
Concentration of the graphene oxide in distilled water in the step 1 is 30g/L, and the addition of the dispersant is oxygen
The 15% of graphite alkene quality, the dispersant use polyvinylpyrrolidone.
The dispersion frequency of ultrasonic disperse in the step 1 is 8kHz, and temperature is 60 DEG C.
For the microwave power of microwave pressurization in the step 2 for 700W, temperature is 150 DEG C, pressure 5MPa, described quick
The speed of pressure release is 0.7MPa/min.
Sodium chloride addition in the step 3 is the 50% of graphene oxide quality, and the methanol addition is distillation
The 60% of water volume.
The voltage of cell reaction in the step 3 be 60V, electric current 90mA, temperature 60 C.
The supersonic frequency of ultrasonic disperse in the step 4 is 15kHz, and temperature is 90 DEG C.
The pressure of sealing pressing reaction in the step 4 is 30MPa, and temperature is 110 DEG C, the pressure release of the quick pressure releasing
Temperature is 100 DEG C, and pressure release speed is 2MPa/min.
Ultrasonic reaction in the step 5 is reacted using water bath sonicator, supersonic frequency 8kHz, and temperature is 70 DEG C,
Drying temperature in the step 5 is 90 DEG C.
Embodiment 3
A kind of electrolytic reduction for preparing graphene, the electrolytic reduction is in accordance with the following steps：
Step 1, graphene oxide particle is put into distilled water, adds in dispersant ultrasonic disperse, obtain graphene oxide
Dispersion liquid；
Step 2, graphene dispersing solution is added in into the microwave compressive reaction 4h into sealing reaction kettle, is obtained after quick pressure releasing thin
Granular graphite alkene dispersion liquid；
Step 3, sodium chloride is added in fine grained graphite alkene dispersion liquid, adds in methanol and stir evenly rear cell reaction 7h,
Obtain graphene dispersing solution；
Step 4, by graphene dispersing solution ultrasonic disperse 2h, then sealing pressing reaction 2h, quick pressure releasing obtain graphene
Mixed precipitation；
Step 5, graphene mixed precipitation is put into ultrasonic reaction 2h in absolute ethyl alcohol, is dried after filtering and obtain graphene material
Material.
Concentration of the graphene oxide in distilled water in the step 1 is 25g/L, and the addition of the dispersant is oxygen
The 12% of graphite alkene quality, the dispersant use polyvinylpyrrolidone.
The dispersion frequency of ultrasonic disperse in the step 1 is 7kHz, and temperature is 50 DEG C.
For the microwave power of microwave pressurization in the step 2 for 500W, temperature is 140 DEG C, pressure 4MPa, described quick
The speed of pressure release is 0.6MPa/min.
Sodium chloride addition in the step 3 is the 40% of graphene oxide quality, and the methanol addition is distillation
The 55% of water volume.
The voltage of cell reaction in the step 3 be 40V, electric current 60mA, 55 DEG C of temperature.
The supersonic frequency of ultrasonic disperse in the step 4 is 12kHz, and temperature is 85 DEG C.
The pressure of sealing pressing reaction in the step 4 is 25MPa, and temperature is 105 DEG C, the pressure release of the quick pressure releasing
Temperature is 95 DEG C, and pressure release speed is 2MPa/min.
Ultrasonic reaction in the step 5 is reacted using water bath sonicator, supersonic frequency 5kHz, and temperature is 65 DEG C,
Drying temperature in the step 5 is 85 DEG C.
Embodiment 4
A kind of electrolytic reduction for preparing graphene, the electrolytic reduction is in accordance with the following steps：
Step 1, graphene oxide particle is put into distilled water, adds in dispersant ultrasonic disperse, obtain graphene oxide
Dispersion liquid；
Step 2, graphene dispersing solution is added in into the microwave compressive reaction 3h into sealing reaction kettle, is obtained after quick pressure releasing thin
Granular graphite alkene dispersion liquid；
Step 3, sodium chloride is added in fine grained graphite alkene dispersion liquid, adds in methanol and stir evenly rear cell reaction 5h,
Obtain graphene dispersing solution；
Step 4, by graphene dispersing solution ultrasonic disperse 1h, then sealing pressing reaction 1h, quick pressure releasing obtain graphene
Mixed precipitation；
Step 5, graphene mixed precipitation is put into ultrasonic reaction 1h in absolute ethyl alcohol, is dried after filtering and obtain graphene material
Material.
Concentration of the graphene oxide in distilled water in the step 1 is 20g/L, and the addition of the dispersant is oxygen
The 10% of graphite alkene quality, the dispersant use polyvinylpyrrolidone.
The dispersion frequency of ultrasonic disperse in the step 1 is 5kHz, and temperature is 40 DEG C.
For the microwave power of microwave pressurization in the step 2 for 400W, temperature is 120 DEG C, pressure 2MPa, described quick
The speed of pressure release is 0.5MPa/min.
Sodium chloride addition in the step 3 is the 30% of graphene oxide quality, and the methanol addition is distillation
The 50% of water volume.
Cell reaction in the step 3 uses gradient cell reaction, and the Gradient program of the cell reaction is as follows：
The supersonic frequency of ultrasonic disperse in the step 4 is 10kHz, and temperature is 80 DEG C.
The pressure of sealing pressing reaction in the step 4 is 20MPa, and temperature is 100 DEG C, the pressure release of the quick pressure releasing
Temperature is 90 DEG C, and pressure release speed is 1MPa/min.
Ultrasonic reaction in the step 5 is reacted using water bath sonicator, supersonic frequency 2kHz, and temperature is 60 DEG C,
Drying temperature in the step 5 is 80 DEG C.
Embodiment 5
A kind of electrolytic reduction for preparing graphene, the electrolytic reduction is in accordance with the following steps：
Step 1, graphene oxide particle is put into distilled water, adds in dispersant ultrasonic disperse, obtain graphene oxide
Dispersion liquid；
Step 2, graphene dispersing solution is added in into the microwave compressive reaction 5h into sealing reaction kettle, is obtained after quick pressure releasing thin
Granular graphite alkene dispersion liquid；
Step 3, sodium chloride is added in fine grained graphite alkene dispersion liquid, adds in methanol and stir evenly rear cell reaction 8h,
Obtain graphene dispersing solution；
Step 4, by graphene dispersing solution ultrasonic disperse 3h, then sealing pressing reaction 3h, quick pressure releasing obtain graphene
Mixed precipitation；
Step 5, graphene mixed precipitation is put into ultrasonic reaction 3h in absolute ethyl alcohol, is dried after filtering and obtain graphene material
Material.
Concentration of the graphene oxide in distilled water in the step 1 is 30g/L, and the addition of the dispersant is oxygen
The 15% of graphite alkene quality, the dispersant use polyvinylpyrrolidone.
The dispersion frequency of ultrasonic disperse in the step 1 is 8kHz, and temperature is 60 DEG C.
For the microwave power of microwave pressurization in the step 2 for 700W, temperature is 150 DEG C, pressure 5MPa, described quick
The speed of pressure release is 0.7MPa/min.
Sodium chloride addition in the step 3 is the 50% of graphene oxide quality, and the methanol addition is distillation
The 60% of water volume.
Cell reaction in the step 3 uses gradient cell reaction, and the Gradient program of the cell reaction is as follows：
| Voltage | Electric current | Temperature | Time |
| 8V | 15mA | 50℃ | 40min |
| 30V | 40mA | 60℃ | 50min |
| 45V | 70mA | 70℃ | 60min |
| 70V | 120mA | 70℃ | 60min |
| 90V | 0.5A | 70℃ | Remaining time |
The supersonic frequency of ultrasonic disperse in the step 4 is 15kHz, and temperature is 90 DEG C.
The pressure of sealing pressing reaction in the step 4 is 30MPa, and temperature is 110 DEG C, the pressure release of the quick pressure releasing
Temperature is 100 DEG C, and pressure release speed is 2MPa/min.
Ultrasonic reaction in the step 5 is reacted using water bath sonicator, supersonic frequency 8kHz, and temperature is 70 DEG C,
Drying temperature in the step 5 is 90 DEG C.
Embodiment 6
A kind of electrolytic reduction for preparing graphene, the electrolytic reduction is in accordance with the following steps：
Step 1, graphene oxide particle is put into distilled water, adds in dispersant ultrasonic disperse, obtain graphene oxide
Dispersion liquid；
Step 2, graphene dispersing solution is added in into the microwave compressive reaction 4h into sealing reaction kettle, is obtained after quick pressure releasing thin
Granular graphite alkene dispersion liquid；
Step 3, sodium chloride is added in fine grained graphite alkene dispersion liquid, adds in methanol and stir evenly rear cell reaction 7h,
Obtain graphene dispersing solution；
Step 4, by graphene dispersing solution ultrasonic disperse 2h, then sealing pressing reaction 2h, quick pressure releasing obtain graphene
Mixed precipitation；
Step 5, graphene mixed precipitation is put into ultrasonic reaction 2h in absolute ethyl alcohol, is dried after filtering and obtain graphene material
Material.
Concentration of the graphene oxide in distilled water in the step 1 is 25g/L, and the addition of the dispersant is oxygen
The 12% of graphite alkene quality, the dispersant use polyvinylpyrrolidone.
The dispersion frequency of ultrasonic disperse in the step 1 is 7kHz, and temperature is 50 DEG C.
For the microwave power of microwave pressurization in the step 2 for 500W, temperature is 140 DEG C, pressure 4MPa, described quick
The speed of pressure release is 0.6MPa/min.
Sodium chloride addition in the step 3 is the 40% of graphene oxide quality, and the methanol addition is distillation
The 55% of water volume.
Cell reaction in the step 3 uses gradient cell reaction, and the Gradient program of the cell reaction is as follows：
| Voltage | Electric current | Temperature | Time |
| 7V | 13mA | 45℃ | 30min |
| 25V | 35mA | 55℃ | 40min |
| 43V | 65mA | 65℃ | 50min |
| 70V | 110mA | 70℃ | 60min |
| 90V | 0.4A | 70℃ | Remaining time |
The supersonic frequency of ultrasonic disperse in the step 4 is 12kHz, and temperature is 85 DEG C.
The pressure of sealing pressing reaction in the step 4 is 25MPa, and temperature is 105 DEG C, the pressure release of the quick pressure releasing
Temperature is 95 DEG C, and pressure release speed is 2MPa/min.
Ultrasonic reaction in the step 5 is reacted using water bath sonicator, supersonic frequency 5kHz, and temperature is 65 DEG C,
Drying temperature in the step 5 is 85 DEG C.
Performance test
| Carbon content | Thermal conductivity | Light transmittance | |
| Embodiment 1 | 97.2% | 4130W/m·K | 88.1% |
| Embodiment 2 | 97.7% | 4312W/m·K | 88.5% |
| Embodiment 3 | 98.2% | 4541W/m·K | 89.6% |
| Embodiment 4 | 98.8% | 4409W/m·K | 90.1% |
| Embodiment 5 | 98.4% | 4753W/m·K | 90.7% |
| Embodiment 6 | 99.1% | 4819W/m·K | 91.5% |
In conclusion the present invention has the following advantages：
1. the present invention solves the problems, such as that the method that existing electrolytic reduction prepares graphene has pollution with safe, preparation
Method is simple and practicable, can not only ensure the high quality of graphene, and preparation method is environment friendly and pollution-free.
2. the present invention as dispersant, can not only play dispersion effect using polyvinylpyrrolidone, at the same right and wrong from
Subtype high-molecular compound, it is with good stability, it can ensure its stability in electrolytic process.
3. the present invention ensures electrolysis effectiveness in a manner that strong electrolyte is mixed with weak electrolyte, while prevents electrolyte
Energy process causes electrolyte to aoxidize, and pollutes.
4. the present invention can all be dissolved the impurity in graphene as lytic agent using absolute ethyl alcohol, while graphene
It is insoluble, so as to promote the purity of graphene.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
The described technical solution of inventive embodiments.It will be understood by those of ordinary skill in the art that still the present invention can be carried out
Modification or equivalent substitution, to reach identical technique effect；As long as meeting using needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of electrolytic reduction for preparing graphene, it is characterised in that：The electrolytic reduction is in accordance with the following steps：
Step 1, graphene oxide particle is put into distilled water, adds in dispersant ultrasonic disperse, obtain graphene oxide and disperse
Liquid；
Step 2, graphene dispersing solution is added in into the microwave compressive reaction 3-5h into sealing reaction kettle, thin is obtained after quick pressure releasing
Grain graphene dispersing solution；
Step 3, sodium chloride is added in fine grained graphite alkene dispersion liquid, adds in methanol and stir evenly rear cell reaction 5-8h, obtain
To graphene dispersing solution；
Step 4, by graphene dispersing solution ultrasonic disperse 1-3h, then sealing pressing reaction 1-3h, quick pressure releasing obtain graphene
Mixed precipitation；
Step 5, graphene mixed precipitation is put into ultrasonic reaction 1-3h in absolute ethyl alcohol, is dried after filtering and obtain graphene material
Material.
2. a kind of electrolytic reduction for preparing graphene according to claim 1, it is characterised in that：In the step 1
Concentration of the graphene oxide in distilled water is 20-30g/L, and the addition of the dispersant is the 10- of graphene oxide quality
15%, the dispersant uses polyvinylpyrrolidone.
3. a kind of electrolytic reduction for preparing graphene according to claim 1, it is characterised in that：In the step 1
The dispersion frequency of ultrasonic disperse is 5-8kHz, and temperature is 40-60 DEG C.
4. a kind of electrolytic reduction for preparing graphene according to claim 1, it is characterised in that：In the step 2
The microwave power of microwave pressurization is 400-700W, and temperature is 120-150 DEG C, pressure 2-5MPa, the speed of the quick pressure releasing
For 0.5-0.7MPa/min.
5. a kind of electrolytic reduction for preparing graphene according to claim 1, it is characterised in that：In the step 3
Sodium chloride addition is the 30-50% of graphene oxide quality, and the methanol addition is the 50-60% of distilled water volume.
6. a kind of electrolytic reduction for preparing graphene according to claim 1, it is characterised in that：In the step 3
The voltage of cell reaction be 30-60V, electric current 30-90mA, 50-60 DEG C of temperature.
7. a kind of electrolytic reduction for preparing graphene according to claim 1, it is characterised in that：In the step 4
The supersonic frequency of ultrasonic disperse is 10-15kHz, and temperature is 80-90 DEG C.
8. a kind of electrolytic reduction for preparing graphene according to claim 1, it is characterised in that：In the step 4
The pressure of sealing pressing reaction is 20-30MPa, and temperature is 100-110 DEG C, and the pressure release temperature of the quick pressure releasing is 90-100
DEG C, pressure release speed is 1-2MPa/min.
9. a kind of electrolytic reduction for preparing graphene according to claim 1, it is characterised in that：In the step 5
Ultrasonic reaction is reacted using water bath sonicator, supersonic frequency 2-8kHz, and temperature is 60-70 DEG C,
10. a kind of electrolytic reduction for preparing graphene according to claim 1, it is characterised in that：In the step 5
Drying temperature is 80-90 DEG C.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101634032A (en) * | 2009-08-14 | 2010-01-27 | 南京大学 | Green and fast electrochemical preparation method for graphene |
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| CN101634032A (en) * | 2009-08-14 | 2010-01-27 | 南京大学 | Green and fast electrochemical preparation method for graphene |
| CN105088261A (en) * | 2014-05-14 | 2015-11-25 | 国能纳米科技有限公司 | Preparation method of graphene |
| CN104894594A (en) * | 2015-05-26 | 2015-09-09 | 广东烛光新能源科技有限公司 | Graphene preparation method |
| CN106591871A (en) * | 2016-12-01 | 2017-04-26 | 燕园众欣纳米科技（北京）有限公司 | Method for preparing graphene through electrochemical in-situ oxidation and reduction |
| CN106676562A (en) * | 2016-12-13 | 2017-05-17 | 西安交通大学 | Method for preparing high-quality graphene through electrochemical reduction |
| CN106587027A (en) * | 2017-01-05 | 2017-04-26 | 苏州高通新材料科技有限公司 | Method for rapidly preparing small-dimensional graphene |
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